Development And Certification Of Candidate Reference Material For TEGDN And DEGDN

Triethylene glycol dinitrate(TEGDN)and diethylene glycol dinitrate(DEGDN)are energetic plasticizers that are widely used in formulations of propellant.They have good application prospects due to their excellent mechanical properties and high energy.Reference materials are the foundation of quality assurance during the analysis process,which are used to calibrate equipments and evaluate analytical testing methods.However,there is no high-purity reference material for TEGDN and DEGDN in domestic at present.This restricts the development of the corresponding analytical technology,and lead to the quality of related products can not be effectively controlled.In order to ensure the accuracy of value traceability and transmission of TEGDN and DEGDN reference materials in production and application,it is especially necessary and urgent to carry out study on the development and certification of TEGDN and DEGDN candidate reference material.The main study contents of this thesis are as follows:1.The candidate reference material TEGDN and DEGDN were prepared with diethylene glycol,triethylene glycol,nitric acid and sulfuric acid by mixed esterification.The reactants dosages,reaction time,reaction temperature and so on have been optimized to select the optimum process conditions.The main components of TEGDN and DEGDN were qualitatively analyzed by infrared spectroscopy,nuclear magnetic resonance and mass spectrometry.2.The analytical methods of impurity components in the candidate reference material TEGDN and DEGDN were established and studied.A gas chromatography-tandem mass spectrometric method was established for the determination of organic impurities.The optimal chromatographic conditions were determined.Organic impurities were qualitatively determined by retrieving the NIST library,comparing with the authentic samples and analyzing formation mechanism of impurities.An external standard method was used to determine the contents of the identified organic impurities.A preparative chromatography-ion chromatography method for the determination of anionic impurities was established.Preparative chromatography was used as a pretreatment method to remove organic compounds from the samples.The anion impurities were effectively separated and collected,and the anion impurities were qualitatively and quantitatively analyzed by ion chromatography.The inorganic element impurities were determined by inductively coupled plasma mass spectrometry.The water in TEGDN and DEGDN was determined by quantitative nuclear magnetic resonance method.3.The purity of the candidate reference material TEGDN and DEGDN was determined by mass balance method and quantitative nuclear magnetic resonance method.The main component of the candidate reference material was determined by gas chromatography method,and the chromatographic conditions were optimized to obtain the best separation conditions.The results of the two certification methods were compared and verified,and the average value was taken as the final purity value.The purity values of the candidate reference material TEGDN and DEGDN were 99.19% and 99.14%,respectively.The homogeneity,long-term stability and short-term stability of the candidate reference material TEGDN and DEGDN were investigated by gas chromatography method.The results show that the two candidate reference material have good homogeneity and stability.